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Method for modifying lignin in eutectic solvent through quaternization

A technology of quaternization modification and deep eutectic solvent, applied in the production of bulk chemicals, etc., can solve the problems of using toxic reagents and harsh reaction conditions, and achieve the effect of easy control of reaction conditions and simple operation methods

Inactive Publication Date: 2014-04-23
NORTHEAST FORESTRY UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problems of using toxic reagents and harsh reaction conditions in existing lignin quaternization modification experiments, the present invention provides a method for quaternization modification of lignin using a deep eutectic solvent as a solvent and reagents, The method is safe and environmentally friendly, and the operating conditions are easy to control. The prepared quaternized modified lignin can be used as a flocculant for dye solutions, etc.

Method used

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  • Method for modifying lignin in eutectic solvent through quaternization

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Embodiment 1

[0014] Example 1. Vacuum-dry choline chloride and urea at 80°C for 12 hours, accurately weigh a certain mass of choline chloride and urea at a molar ratio of 1:2, and stir magnetically at 80°C until Light yellow transparent liquid, enzymatic lignin is added to 0.1mol / L sodium hydroxide solution at a mass ratio of 20:100, after the lignin is completely dissolved, 1mol / L hydrochloric acid is added drop by drop under stirring until the pH value of the solution is 1 ~2, keep warm at 70°C for 30 minutes, filter, wash with water, and dry to obtain purified lignin. Add 0.1g of purified lignin to 5g of deep eutectic solvent, add 0.4g of sodium hydroxide after the lignin is dissolved, and react at 90°C for 5h, and after the reactant is cooled, add 20g of potassium ferricyanide with a mass fraction of 10% The aqueous solution is filtered, washed with water and dried to obtain quaternized modified lignin.

Embodiment 2

[0015] Example 2, vacuum-dry choline chloride and urea at 80°C for 12 hours, accurately weigh a certain mass of choline chloride and urea at a molar ratio of 1:2, and stir magnetically at 80°C until Light yellow transparent liquid, enzymatic lignin is added to 0.1mol / L sodium hydroxide solution at a mass ratio of 20:100, after the lignin is completely dissolved, 1mol / L hydrochloric acid is added drop by drop under stirring until the pH value of the solution is 1 ~2, keep warm at 70°C for 30 minutes, filter, wash with water, and dry to obtain purified lignin. Add 0.3g of purified lignin to 5g of deep eutectic solvent, add 0.4g of sodium hydroxide after the lignin is dissolved, and react at 90°C for 10h, and after the reactant is cooled, add 20g of potassium ferricyanide with a mass fraction of 10% The aqueous solution is filtered, washed with water and dried to obtain quaternized modified lignin.

Embodiment 3

[0016] Example 3. Vacuum-dry choline chloride and urea at 80°C for 12 hours, accurately weigh a certain mass of choline chloride and urea at a molar ratio of 1:2, and stir magnetically at 80°C until Light yellow transparent liquid, enzymatic lignin is added to 0.1mol / L sodium hydroxide solution at a mass ratio of 20:100, after the lignin is completely dissolved, 1mol / L hydrochloric acid is added drop by drop under stirring until the pH value of the solution is 1 ~2, keep warm at 70°C for 30 minutes, filter, wash with water, and dry to obtain purified lignin. Add 0.5g of purified lignin to 5g of deep eutectic solvent, add 0.4g of sodium hydroxide after the lignin is dissolved, react at 90°C for 20h, and after the reactant is cooled, add 20g of potassium ferricyanide with a mass fraction of 10% The aqueous solution is filtered, washed with water and dried to obtain quaternized modified lignin.

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Abstract

The invention relates to a method for modifying lignin in an eutectic solvent chloro choline chloride / urea through quaternization. The method comprises steps of firstly, preparing the eutectic solvent; secondly, purifying the lignin; thirdly, dissolving the lignin in the eutectic solvent, adding a catalyst for quaterisation; and fourthly, after cooling down the reactant, adding an excess potassium ferricyanide water solution, filtering, washing, and drying so as to obtain the lignin modified through quaternization. The eutectic solvent is used as both the solvent and reagent for quaterisation so as to modify the lignin and is non-toxic and harmless compared with traditional quaterisation. The lignin modified through quaternization can be used as functional materials such as flocculating agent, surfactant, emulgator, oil-displacing agent, water reducer and the like.

Description

technical field [0001] The invention belongs to the field of high-efficiency utilization of natural polymer resources, and in particular relates to a method for quaternizing modified lignin in a deep eutectic solvent. Background technique [0002] Lignin is the second most abundant natural material on earth after cellulose. The pulp and paper industry produces a large amount of lignin every year, but most of the lignin is discharged or incinerated in the form of "black liquor", which cannot be efficiently utilized; with the gradual development of bioethanol technology, the output of lignin residues will decrease. will increase year by year. Making full use of lignin resources can not only reduce environmental pollution, but also reduce the cost of pulp and paper industry and bioethanol industry. Lignin contains many active groups, such as hydroxyl, carboxyl, benzyl, methoxy, aldehyde, etc., so some chemical modifications can be performed on lignin, such as sulfonation modi...

Claims

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Application Information

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IPC IPC(8): C08H7/00
CPCY02P20/54
Inventor 李利芬胡英成
Owner NORTHEAST FORESTRY UNIVERSITY
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